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Thermoplastic Forming of Metallic Glass: Die Selection, Microforming and Property Characterisation

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Thermoplastic Forming of Metallic Glass: Die Selection, Microforming and Property Characterisation Thermoplastic Forming of Metallic Glass: Die Selection, Microforming and Property Characterisation Thesis by Amir Monfared A Thesis in Fulfilment of the Requirements for the Degree of Doctor of Philosophy School of Mechanical and Manufacturing Engineering The University of New South Wales Sydney, Australia August 2018 PLEASE TYPE THE UNIVERSITY OF NEW SOUTH WALES Thesis/Dissertation Sheet Surname or Family name: Monfared First name: Amir Other name/s: ;. Abbreviation for degree as given in the University calendar: PhD School: Mechanical and Manufacturing Faculty: Engineering Title: Thermoplastic Forming of Metallic Glass: Die Selection, Microforming and Property Characterisation Abstract 350 words maximum: (PLEASE TYPE) Metallic glass (MG) is a promising class of materials with exceptional properties. Due to non-equilibrium amorphous structure, manufacturing of these alloys is challenging and might lead to structural and properties changes. Thermoplastic forming (TPF) is an efficient manufacturing technique of MGs. However, there are still many challenges (e.g. MG/die adhesion) and ambiguities such as the effect of TPF on apparent viscosity, mechanical property and structure which should be resolved. Accordingly, this thesis aims to examine TPF of MGs and improve the manufacturing of these alloys. The following lists the major findings of this thesis: 1) The dies with lower surface free energy (SFE) and higher bonding dissociation energy showed the least adhesion with MGs. Chemical adhesion and diffusionwere recognized as the primary adhesion mechanisms. New models were developed and verified for the evaluation of SFE of MGs and the work of adhesion between MGs and dies. 2) Apparent viscosity investigations revealed that at lower temperatures the apparent viscosity increased throughout the tests. However, at higher temperatures viscosity reached to a plateau. 3) The structural analyses of MGs revealed that TPF altered the diffractionpatterns size. The diameter size of the first ring of diffractionpattern increased afterTPF; yet the diameter size becomes larger with temperature. Due to the inverse relationship of interatomic spacing and ring size in diffractiontheory, it was concluded that interatomic spacing reduced after TPF confirming free volume annihilation. DSC analyses showed that the heat release of the sample thermoplastically formed is smaller than the as­ received MG; yet heat release decreases with increasing forming temperature. This verifies the occurrence of structural relaxation during TPF. 4) It was found that MGs becomes harder afterTPF; yet, the hardness increases with temperature rise. It was also demonstrated that dies played trivial role in the hardening of MGs. It was revealed that the load displacement curves of the samples after TPF exhibited less pop-ins compared with the as-received MGs. Based on viscosity variation, HRTEM analyses, DSC investigations and nanoindentation results, free volume annihilation via structural relaxation was identifiedas the primary hardening mechanism. Declaration relating to disposition of project thesis/dissertation I hereby grant to the University of New South Wales or its agents the right to archive and to make available my thesis or dissertation in whole or in part in the University libraries in all forms of media, now or here after known, subject to the provisions of the Copyright Act 1968. I retain all property rights, such as patent rights. I also retain the right to use in future works (such as articles or books) all or part of this thesis or dissertation. I also authorise University Microfilms to use the 350 word abstract of my thesis in DissertationAbstracts International (this is applicable to doctoral theses only) . ....... .......................... ........ wJness Signature . 2.J/?/2-PloDate The University recognises that there may be exceptional circumstances requiring restrictions on copying or conditions on use. Requests for restriction for a period of up to 2 years must be made in writing. Requests for a longer period of restriction may be considered in exceptional circumstances and re uire the a roval of the Dean of Graduate Research. FOR OFFICE USE ONLY Date of completion of requirements for Award: Acknowledgement Firstly, I would like to express my sincere gratitude to my supervisor Professor Liangchi Zhang for the continuous support of my Ph.D study and related research, his patience, encouragement, advice and immense knowledge. His guidance helped me in all the time of research and writing of this thesis. I also express my deepest gratitude to my co-supervisor, Dr. Weidong Liu for his unselfish help and patience, guidance and crucial advice at different stages of the research, without whose assistance, this study would not have been successful. I would like to thank all of the members of the Laboratory for Precision and Nano Processing Technologies (LPNPT) for stimulating discussions and their assistance during experimentations in the past four years. Last but not the least; I would like to thank my family: my parents and my brother for supporting me spiritually throughout writing this thesis and my life in general. i Abstract Metallic glass (MG) is a promising class of material with exceptional properties. Due to non-equilibrium amorphous structure; manufacturing of these alloys is challenging and can lead to changes in structure and properties. Thermoplastic forming (TPF) is one of the most efficient manufacturing techniques of MGs. However, due to amorphous structure in the supercooled liquid region (SCLR), crystallisation and property changes are likely to occur in TPF. While some research has been conducted in this area, there are still many challenges and ambiguities (e.g. MG/die adhesion, apparent viscosity changes in TPF, effect of TPF on mechanical property and structure of MG) that should be addressed to obtain a technique with higher performance. Adhesion significantly affects the quality of manufacturing and net price of production through deteriorating the surface quality of MG and die. Apparent viscosity plays a major role in TPF; however comprehensive research examining apparent viscosity variation in TPF is lacking. Apparent viscosity is important in revealing the deformation behaviour of MG in TPF. In addition, the effect of TPF on the structure and mechanical property of MGs remains unclear. Given the importance of MG structure and property on the performance of MGs in service, exploring the structure and property of MGs after TPF is essential. Thus, this thesis aims to examine the TPF of MGs to address the challenges and ambiguities in this area and improve the efficiency of manufacturing of MGs. The major findings of this thesis are listed as follow: 1) Several materials including electroless Ni-P, Si, SiC, Si3N4, alumina, polytetrafluoroethylene (PTFE), sapphire and WC-Co were employed to examine ii their adhesion status with La-based and Zr-based MGs. It was revealed that WC- Co, sapphire and PTFE had the lowest adhesion status. Among these three materials, WC-Co was identified as the best die due to its superior machinability, excellent mechanical properties, higher working temperature and cheaper price. 2) Surface free energy (SFE) and bonding dissociation energy (BDE) of the dies were identified as the parameters playing the major roles in the adhesion status. The dies with lower SFE and higher BDE showed the least adhesion with MGs and vice versa. Chemical adhesion and diffusion were recognised as the primary adhesion mechanisms in TPF, as verified through energy dispersive spectroscopy analyses and high resolution scanning electron microscope observations. 3) Due to the importance of SFE in TPF of MGs and the lack of appropriate model in this area, a new model was developed in this thesis for the evaluation of SFE of MGs and was verified with the available experimental data. In addition, a novel model was introduced in this thesis for estimation of the work of adhesion between MGs and dies and its validity was verified through the experimental observations. 4) Given the importance of apparent viscosity in TPF, the apparent viscosity variation of MG during TPF at different temperatures has been obtained in this thesis. At lower temperatures where viscosity is far from equilibrium, the apparent viscosity increased throughout the tests. However, at higher temperatures where the apparent viscosity approaches equilibrium, viscosity reaches a plateau with little variation. Viscosity variation demonstrates the free volume annihilation in TPF. 5) The structure of MGs before and after TPF were thoroughly analysed through X- ray diffraction and high resolution transmission electron microscope (HRTEM). iii The analyses verified the amorphous structure of MG after TPF at all temperatures. However it was revealed that TPF altered the diffraction patterns. The diameter size of the first ring of diffraction pattern increased after TPF; yet the diameter size became larger with temperature rise. Due to the inverse relationship between interatomic spacing and ring size in diffraction theory, it was concluded that interatomic spacing reduced after TPF, thus confirming free volume annihilation through structural relaxation. 6) Differential scanning calorimetry (DSC) analyses of the as-received and thermoplastically formed sample revealed the occurrence of structural relaxation. By comparison with the as-received MG, heat release decreased for the sample thermoplastically formed and decreased further with increasing the forming temperature.
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